CN115188607A - Defective Fe 3 O 4 @ Fe electrode material and preparation method thereof - Google Patents
Defective Fe 3 O 4 @ Fe electrode material and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to defective Fe 3 O 4 @ Fe electrode material and preparation method thereof, in particular to Fe electrode material prepared by regulating annealing temperature and reducing method 3 O 4 The surface of the @ Fe electrode material is modified. The electrode material prepared by the method can obtain more oxygen vacancies and expose more electrochemical active sites, and can be applied to the fields of supercapacitors and electrochemical catalysis.
Description
Technical Field
The invention relates to the field of electrode materials of supercapacitors, in particular to defective Fe 3 O 4 A @ Fe electrode material and a preparation method thereof.
Background
Due to the over-depletion of fossil fuels, coupled with the increasing environmental degradation, considerable efforts are currently being made to develop advanced electrochemical energy storage and conversion systems. And the supercapacitor and electrocatalytic water splitting hydrogen production technologies have received much attention as representative technologies for solving the above problems. Among them, super capacitor is a typical energy storage device, and has attracted great interest due to its high power density, long life, safety and reliability. These characteristics make supercapacitors indispensable in applications where frequent and rapid storage and release of electrical energy is required.
However, one drawback of supercapacitors to date is the lack of energy density, which severely hampers their practical application. Meanwhile, electrocatalytic decomposition of water is one of the effective ways to provide hydrogen fuel. However, the Oxygen Evolution Reaction (OER) is its major bottleneck, and the process kinetics are slow, resulting in an overall inefficient hydrogen production. Although iridium-based and ruthenium-based catalysts have shown excellent electrochemical performance, their high cost and scarcity have limited their large-scale application. Therefore, the search for low cost, high efficiency bifunctional electrode materials is the key to the development of advanced electrochemical energy storage and conversion devices.
In transition metal oxides for supercapacitors, fe 3 O 4 Due to its high theoretical specific capacitance, good electrochemical activity, abundant supply of materials and environmental friendliness, it has attracted research interest in recent years. However, most of the time Fe is due to the low electron conductivity and polarization loss during cycling 3 O 4 The specific capacitance observed for the electrodes is much lower than the theoretical value, which makes them unsuitable for large-scale applications.
For this reason, those skilled in the art wish to develop a high-performance Fe 3 O 4 The electrode material can obtain more oxygen vacancies, expose more electrochemical active sites and improve Fe 3 O 4 Electrochemical performance of the electrode material.
Disclosure of Invention
It is an object of the present invention to overcome the disadvantages of the prior art, and in a first aspect to provide a deficient Fe 3 O 4 The method for preparing the @ Fe electrode material obtains the electrode material with a large number of oxygen defects and more electrochemistry through annealing treatment and reduction treatment of Prussian blue in sequenceHigh performance Fe of active site 3 O 4 @ Fe electrode material.
In order to achieve the above purpose, the invention provides the following technical scheme:
defective Fe 3 O 4 The preparation method of the @ Fe electrode material comprises the following steps of:
preparing prussian blue; and
and sequentially carrying out annealing treatment and reduction treatment on the Prussian blue.
Preferably, the temperature of the annealing treatment is 600-1200 ℃, such as 600 ℃, 800 ℃, 900 ℃, 1000 ℃, 1200 ℃ and the like; preferably 800 deg.C, 900 deg.C, 1000 deg.C.
Preferably, the temperature rise rate of the annealing treatment is 2-5 min/DEG C, preferably 5 min/DEG C.
Preferably, the time of the annealing treatment is 1 to 5 hours, preferably 2 to 3 hours.
Preferably, the reducing agent for the reduction treatment is NaBH 4 。
Preferably, the time of the reduction treatment is 10-30min, preferably 20-30min. The proper reduction treatment time greatly improves the material performance.
According to the technical scheme of the invention, the defect type Fe embedded in the metal Fe particle is quickly synthesized through the solid pyrolysis conversion process of the Prussian blue 3 O 4 @ Fe electrode material, followed by NaBH 4 And (3) performing reduction treatment to obtain the electrode material which has a large number of oxygen defects and exposes more electrochemical active sites and has higher electrochemical activity.
Reduced defective Fe 3 O 4 The @ Fe electrode material has obvious change in shape, the connected polyhedron is dispersed, the particle size is obviously reduced, a large number of uniform nanosheets are generated on the surface of the polyhedron to form an interconnected network structure, the specific surface area is increased, the diffusion and transmission path of ionic electrons are shortened, the rapid transmission of electrolyte ions is improved, and the electrochemical property is promoted.
Preferably, the preparation method of the prussian blue comprises the following steps:
uniformly mixing a potassium ferrocyanide solution and a ferric chloride solution to obtain a mixed solution; and stirring, cleaning and drying the mixed solution in sequence to obtain the Prussian blue.
Preferably, in the mixed solution, the molar ratio of potassium ferrocyanide to ferric chloride is (1-3): (4-8).
Preferably, the stirring is magnetic stirring.
Preferably, the magnetic stirring time is 0.5 to 2 hours, preferably 1.5 to 2 hours.
Preferably, the drying is freeze drying.
Preferably, the drying temperature is-70 to-40 ℃, preferably-60 to-40 ℃, and the drying time is 12 to 24 hours, preferably 18 to 24 hours.
In a second aspect, the invention provides a defective Fe prepared by the preparation method of the first aspect 3 O 4 @ Fe electrode material.
In a third aspect, the invention provides an electrode comprising said deficient Fe 3 O 4 @ Fe electrode material.
Preferably, the electrode comprises a substrate and defective Fe disposed on the substrate 3 O 4 @ Fe electrode material.
Preferably, the substrate is a foamed nickel substrate.
Preferably, the foamed nickel substrate is pretreated by:
and (3) carrying out ultrasonic cleaning on the foamed nickel substrate in hydrochloric acid, ethanol and deionized water in sequence, and then carrying out drying treatment.
The invention provides a super capacitor, which comprises the electrode.
Compared with the prior art, the invention has the beneficial effects that:
1. defective Fe prepared by the invention 3 O 4 The @ Fe electrode material can obtain more oxygen vacancies and expose more electrochemical active sites, thereby obtaining better electrochemical performance.
2. Preparation of the inventionDefective Fe obtained 3 O 4 The @ Fe-900-20 electrode material has good wettability in water, is favorable for effective diffusion of electrode liquid ions, and improves the electrochemical reaction rate.
3. The preparation process is efficient, safe and environment-friendly.
Drawings
FIG. 1 shows defective Fe prepared by the present invention 3 O 4 Scanning Electron Microscope (SEM) images of @ Fe electrode material; wherein (a-b) is Fe 3 O 4 SEM photograph of @ Fe-900 electrode material; (c-d) is Fe 3 O 4 SEM photograph of the electrode material of @ Fe-900-20.
FIG. 2 shows defective Fe prepared by the present invention 3 O 4 XRD and XPS spectrograms of @ Fe electrode material; wherein (a-b) is Prussian Blue (PB) and Fe 3 O 4 The XRD pattern of @ Fe electrode material; (c-d) is Fe 3 O 4 XPS spectra of @ Fe electrode material.
FIG. 3 is a test chart of electrochemical performance of different electrode materials; wherein (a) is a CV curve comparison; (b) comparing charge and discharge curves; (c) comparing the specific capacitance under different current densities; (d) EIS comparison chart; and (e) comparing the cycling stability.
FIG. 4 is a graph of the HER and OER performance tests of supercapacitor electrodes using different electrode materials; (a) is a HER curve; (b) Is at 10mA · cm -2 At 10 and 30mA cm -2 A graph of HER overpotential versus current density; (c) is OER curve; (d) At 30mA · cm -2 And 50mA · cm -2 OER overpotential contrast plot at current density.
Detailed Description
In order to facilitate understanding of the present invention, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention. Unless otherwise indicated, the starting materials and reagents used in the examples are all commercially available products. Reagents, equipment, or procedures not described herein are routinely determinable by a person of ordinary skill in the art.
Example 1
This example provides a deficient Fe 3 O 4 The @ Fe-800-20 electrode material is prepared by the following steps:
1. 4.2239g of potassium ferrocyanide and 10.812g of ferric chloride are dissolved in 20ml of deionized water and 80ml of deionized water respectively, and the mixture is stirred uniformly to obtain light yellow and orange yellow solutions respectively.
2. And (3) mixing the two solutions in the step (1), magnetically stirring for 1.5h at room temperature to obtain a deep blue uniform solution, repeatedly cleaning the solution by using deionized water, and freeze-drying the solution for 24h at the temperature of-55 ℃ to obtain Prussian blue powder.
3. Pyrolyzing the Prussian blue powder prepared in the step 2 at 800 ℃ for 2h at the heating rate of 5 ℃/min, and then using NaBH 4 Treating for 20 minutes to obtain defective Fe 3 O 4 @ Fe-800-20 electrode material.
Example 2
This example provides a deficient Fe 3 O 4 The @ Fe-900-20 electrode material is prepared by the following steps:
1. 4.2239g of potassium ferrocyanide and 10.812g of ferric chloride are dissolved in 20ml of deionized water and 80ml of deionized water respectively, and the mixture is stirred uniformly to obtain light yellow and orange yellow solutions respectively.
2. And (3) mixing the two solutions in the step (1), magnetically stirring for 1.5h at room temperature to obtain a deep blue uniform solution, repeatedly cleaning the solution by using deionized water, and freeze-drying the solution for 24h at the temperature of-55 ℃ to obtain Prussian blue powder.
3. Pyrolyzing the Prussian blue powder prepared in the step 2 at 900 ℃ for 2h, wherein the heating rate is 5 ℃/min, and then using NaBH 4 Treating for 20 min to obtain defective Fe 3 O 4 @ Fe-900-20 electrode material.
Example 3
This example provides a deficient Fe 3 O 4 The @ Fe-1000-20 electrode material is prepared by the following steps:
1. 4.2239g of potassium ferrocyanide and 10.812g of ferric chloride are dissolved in 20ml of deionized water and 80ml of deionized water respectively, and stirred uniformly to obtain light yellow and orange yellow solutions respectively.
2. And (3) mixing the two solutions in the step (1), magnetically stirring for 1.5h at room temperature to obtain a deep blue uniform solution, repeatedly cleaning the solution by using deionized water, and freeze-drying the solution for 24h at the temperature of-55 ℃ to obtain Prussian blue powder.
3. Pyrolyzing the Prussian blue powder prepared in the step 2 at 1000 ℃ for 2h at the heating rate of 5 ℃/min, and then using NaBH 4 Treating for 20 minutes to obtain defective Fe 3 O 4 @ Fe-1000-20 electrode material.
Comparative example 1
The same procedure as in example 1 was used. Except that comparative example 1 did not carry out NaBH in step 3 4 Treating to prepare Fe 3 O 4 @ Fe-800 electrode material
Comparative example 2
The same procedure as in example 2 was used. Except that comparative example 2 did not carry out NaBH in step 3 4 Treating to prepare Fe 3 O 4 @ Fe-900 electrode material.
Comparative example 3
The same procedure as in example 3 was used. Except that comparative example 3 did not carry out NaBH in step 3 4 Treating to prepare Fe 3 O 4 @ Fe-1000 electrode material.
Experimental example 1
Scanning electron microscope imaging was performed on the electrode materials prepared in example 2 and comparative example 2.
The imaging results are shown in fig. 1. According to FIG. 1, it can be seen that: FIG. 1 (a-b) shows the original Fe 3 O 4 The @ Fe-900 electrode material is a micron-sized cluster structure formed by connecting polyhedrons, and the particle size is about 5 microns. As can be seen from FIG. 1 (c-d), the NaBH is passed 4 After being treated for 20 minutes, the shape of the electrolyte is obviously changed, the connected polyhedrons are dispersed, the particle size is obviously reduced to be about 2.5 microns, and meanwhile, a large number of uniform nano sheets are generated on the surfaces of the polyhedrons to form an interconnected network structure, so that the specific surface area is increased, the diffusion and transmission path of ionic electrons is shortened, and the electrolyte is improvedThe rapid transmission of ions is beneficial to the improvement of electrochemical properties.
Experimental example 2
XRD and XPS tests were performed on Prussian Blue (PB) and the electrode materials prepared in example 3, comparative example 1, comparative example 2, and comparative example 3.
The test results are shown in fig. 2. The phase and crystallinity of the prussian blue and the electrode material were analyzed by XRD, and as can be seen from fig. 2 (a), the characteristic peak of the synthesized prussian blue and Fe 4 (Fe(CN) 6 ) 3 (JCPDS 73-0687) match well, which demonstrates the success of Prussian blue synthesis. As can be seen from FIG. 2 (b), fe 3 O 4 @Fe-800、Fe 3 O 4 @Fe-900、 Fe 3 O 4 @Fe-1000、Fe 3 O 4 Characteristic peaks of @ Fe-900-20 electrode material and Fe 3 O 4 (JCPDS 79-0419) are matched, and diffraction peaks at 18.2 degrees, 30.0 degrees, 35.4 degrees, 37.0 degrees, 43.0 degrees, 53.4 degrees, 56.9 degrees, 62.5 degrees and 74.9 degrees respectively correspond to Fe 3 O 4 The (111), (220), (311), (222), (400), (422), (511), (440), and (622) planes of (a). In particular, fe increases with the calcination temperature 3 O 4 Gradually decreases in diffraction peak of Fe at a calcination temperature of 1000 deg.C 3 O 4 The @ Fe-1000 electrode material shows a diffraction peak related to C (JCPDS 75-2078), which indicates that the sample is likely to be carbonized seriously when the annealing temperature is too high. At the same time, fe 3 O 4 @Fe-800、Fe 3 O 4 @Fe-900、Fe 3 O 4 The @ Fe-1000 electrode material also has a diffraction peak corresponding to Fe (JCPDS 87-0721). FIG. 2 (c-d) shows more clearly the passage of NaBH 4 Treated Fe 3 O 4 The @ Fe-900-20 electrode material has more oxygen vacancies, which may ensure rapid electron transfer to achieve desirable electrochemical performance.
Experimental example 3
And preparing electrodes by respectively adopting the electrode materials prepared in the embodiment 3 and the comparative examples 1, 2 and 3, assembling the electrodes into a super capacitor, and testing the performances of the electrodes and the super capacitor.
The preparation method of the electrode comprises the following steps:
the prepared defective Fe 3 O 4 The @ Fe electrode material is disposed on a foamed nickel substrate. The foamed nickel substrate was pretreated as follows:
cutting foamed nickel into 1 × 2cm 2 The piece is sequentially subjected to ultrasonic cleaning in 3M hydrochloric acid, ethanol and deionized water for 10 minutes, and then the processed foam nickel is placed in a 60-degree oven for drying treatment, so that the cleaned foam nickel substrate material is finally obtained.
The prepared defective Fe 3 O 4 Uniformly mixing the @ Fe electrode material, polyvinylidene fluoride (PVDF) and conductive carbon black according to the mass ratio of 8 2 And preparing the electrode slice. And (3) placing the electrode slice in a constant-temperature vacuum drying oven at 60 ℃ for drying for 12h to prepare the electrode. Finally, tabletting and weighing are carried out, and the loading capacity of the four defective Fe3O4@ Fe electrode materials is about 3mg cm -2 。
The preparation method of the super capacitor comprises the following steps:
asymmetric ultracapacitor: defective Fe3O4@ Fe electrode material is selected as a positive electrode material, activated carbon for a super capacitor is selected as a negative electrode material, and 3 mol.L -1 The KOH aqueous solution is used as electrolyte, and the materials are assembled into the asymmetric super capacitor.
Determination of electrochemical properties:
in the three-electrode system of the experimental example, a platinum sheet, a mercury/mercury oxide electrode, and a KOH aqueous solution with a concentration of 3M were selected as a counter electrode, a reference electrode, and an electrolyte in the test, respectively. Will be defective Fe 3 O 4 The @ Fe electrode material is prepared into an electrode slice serving as a working electrode to test the electrochemical performance of the electrode slice, and the scanning rate is 5mV · s through measurement of Cyclic Voltammetry (CV) within a potential range of 0-0.6V -1 To 50 mV. S -1 . Selecting current density from 1 mA-cm -2 To 10mA cm -2 To carry outConstant current charge and discharge (GCD) test. The testing of electrochemical performance also includes Electrochemical Impedance Spectroscopy (EIS), rate performance, stability testing, and Linear Sweep Voltammetry (LSV) curve testing.
Specific capacitance calculation formula:
i is the current density (mA · cm) -2 ) (ii) a Δ t is the discharge time; s is the area (cm) of the active material participating in the electrochemical reaction -2 ) (ii) a Δ V is the voltage window (V).
The electrochemical performance test patterns of the different electrode materials are shown in fig. 3.
The results of the electrochemical performance test of the electrode are shown in fig. 4.
From the electrochemical performance test results of different electrode materials in fig. 3, it can be seen that: FIG. 3 (a) shows different electrode materials at a sweep rate of 50mV · s -1 CV control of the following, in which Fe 3 O 4 The closed area of the integral curve of @ Fe-900-20 is the largest. From FIG. 3 (b), the electrode material was varied at 1mA cm -2 The same results were obtained in the following comparative charge/discharge graphs, fe 3 O 4 The longest discharge time of @ Fe-900-20. Fig. 3 (c) shows the specific capacitance of different electrode materials at different current densities. The results showed that the current density was 1mA cm -2 When the specific capacitance of the electrode material is 1526.7mF cm, the specific capacitance of the electrode material is Fe3O4@ Fe-900-20 -2 . When the current density increased to 10mA cm -2 Of (i) Fe 3 O 4 The specific capacitance of the electrode material of @ Fe-900-20 is 967.8mF cm -2 . As can be seen in the EIS spectrum of FIG. 3 (d), fe 3 O 4 The @ Fe-900-20 electrode material has the maximum slope, which proves that Fe 3 O 4 The @ Fe-900-20 electrode material has minimal charge transfer resistance. Stability is one of the important indicators for measuring the utility of electrodes. At 5 mA-cm -2 Fe prepared under the condition of 3000 times of circulation of FIG. 3 (e) 3 O 4 @ Fe-900-20 electrode material the electrode retained 92.6% of the initial capacity, while Fe after 3000 cycles 3 O 4 @ Fe-900 electrode materialOnly 87.94% of the initial capacity was reached, indicating Fe 3 O 4 The @ Fe-900-20 electrode material has good cycle stability.
From the electrocatalytic performance test results of fig. 4, it can be seen that: HER activity of the electrodes was studied using Linear Sweep Voltammetry (LSV) with reference to the potential of the hydrogen electrode (RHE), as shown in fig. 4 (a-b). Fe 3 O 4 The LSV data for @ Fe-900-20 shows significant HER performance with very low overpotentials at current densities of 10mA cm -2 223mV at the current density of 30mA cm -2 The overpotential was 311mV. The LSV polarization curves and overpotential contrast plots of FIG. 4 (c-d) show that the polarization is induced by NaBH 4 After treatment, fe 3 O 4 @ Fe-900-20 electrode at a current density of 30mA cm -2 And 50mA · cm -2 When the voltage is higher than the reference voltage, the overpotential is 323mV and 359mV respectively. The improvement in electrochemical performance may be through NaBH 4 A large number of oxygen vacancies are introduced in the treatment, and VO (oxygen vacancy) engineering can effectively improve electron transfer kinetics, increase the electrochemical active sites of the electron transfer, effectively shorten the diffusion transport path of ions and electrons and improve the electrochemical activity.
While the invention has been described with reference to specific preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. Defective Fe 3 O 4 The preparation method of the @ Fe electrode material is characterized by comprising the following steps of:
preparing Prussian blue; and
and sequentially carrying out annealing treatment and reduction treatment on the Prussian blue.
2. Defective Fe according to claim 1 3 O 4 The preparation method of the @ Fe electrode material is characterized in that the annealing treatment temperature is 600-1200 ℃, and the heating rate isIs 2-5 ℃/min.
3. Defective Fe according to claim 2 3 O 4 The preparation method of the @ Fe electrode material is characterized in that the annealing treatment time is 1-5h, preferably 2-3h.
4. Defective Fe according to claim 1 3 O 4 The preparation method of the @ Fe electrode material is characterized in that the reducing agent for reduction treatment is NaBH 4 。
5. Defective Fe according to claim 4 3 O 4 The preparation method of the @ Fe electrode material is characterized in that the time of the reduction treatment is 10-30min, preferably 20-30min.
6. Defective Fe according to claim 1 3 O 4 The preparation method of the @ Fe electrode material is characterized by comprising the following steps of:
uniformly mixing a potassium ferrocyanide solution and a ferric chloride solution to obtain a mixed solution; sequentially stirring, cleaning and drying the mixed solution to prepare Prussian blue;
preferably, in the mixed solution, the molar ratio of potassium ferrocyanide to ferric chloride is (1-3): (4-8).
7. Defective Fe according to claim 6 3 O 4 The preparation method of the @ Fe electrode material is characterized in that the stirring is magnetic stirring;
preferably, the magnetic stirring time is 0.5-2h;
preferably, the drying is freeze-drying;
preferably, the drying temperature is-70 to-40 ℃, and the drying time is 12 to 24 hours.
8. Defective Fe produced by the production method according to any one of claims 1 to 9 3 O 4 @ Fe electrode material.
9. An electrode comprising the electrode material of claim 8.
10. A supercapacitor comprising the electrode of claim 9.
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